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Designation: E1225 13

Standard Test Method for


Thermal Conductivity of Solids Using the Guarded-
Comparative-Longitudinal Heat Flow Technique1
This standard is issued under the fixed designation E1225; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon () indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope 2. Referenced Documents


1.1 This test method describes a steady state technique for 2.1 ASTM Standards:2
the determination of the thermal conductivity, , of E230 Specification and Temperature-Electromotive Force
homogeneous-opaque solids (see Notes 1 and 2). This test (EMF) Tables for Standardized Thermocouples
method is applicable to materials with effective thermal con-
3. Terminology
ductivities in the range 0.2 < < 200 W/(mK) over the
temperature range between 90 and 1300 K. It can be used 3.1 Descriptions of Terms and Symbols Specific to This
outside these ranges with decreased accuracy. Standard:
3.1.1 Terms:
NOTE 1For purposes of this technique, a system is homogeneous if 3.1.1.1 thermal conductivity, the time rate of heat flow,
the apparent thermal conductivity of the specimen, A, does not vary with
changes of thickness or cross-sectional area by more than 65 %. For
under steady conditions, through unit area, per unit temperature
composites or heterogeneous systems consisting of slabs or plates bonded gradient in the direction perpendicular to the area;
together, the specimen should be more than 20 units wide and 20 units 3.1.1.2 apparent thermal conductivitywhen other modes
thick, respectively, where a unit is the thickness of the thickest slab or of heat transfer through a material are present in addition to
plate, so that diameter or length changes of one-half unit will affect the conduction, the results of the measurements performed accord-
apparent A by less than 65 %. For systems that are non-opaque or
partially transparent in the infrared, the combined error due to inhomo- ing to this test method will represent the apparent or effective
geneity and photon transmission should be less than 65 %. Measurements thermal conductivity for the material tested.
on highly transparent solids must be accompanied with infrared absorption 3.1.2 Symbols:
coefficient information, or the results must be reported as apparent thermal
conductivity, A. M(T) = thermal conductivity of meter bars (reference
materials) as a function of temperature, (W/
NOTE 2This test method may also be used to evaluate the contact (mK)),
thermal conductance/resistance of materials.
M1 = thermal conductivity of top meter bar (W/
1.2 The values stated in SI units are to be regarded as (mK)),
standard. No other units of measurement are included in this M2 = thermal conductivity of bottom meter bar (W/
standard. (mK)),
S(T) = thermal conductivity of specimen corrected
1.3 This standard does not purport to address all of the
for heat exchange where necessary, (W/
safety concerns, if any, associated with its use. It is the
(mK)),
responsibility of the user of this standard to establish appro- 'S(T) = thermal conductivity of specimen calculated
priate safety and health practices and determine the applica- by ignoring heat exchange correction, (W/
bility of regulatory limitations prior to use. (mK)),
I(T) = thermal conductivity of insulation as a func-
tion of temperature, (W/(mK)),
1
This test method is under the jurisdiction of ASTM Committee E37 on Thermal
Measurements and is the direct responsibility of Subcommittee E37.05 on Thermo-
2
physical Properties. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2013. Published November 2013. Originally contact ASTM Customer service at service@astm.org. For Annual Book of ASTM
approved in 1987. Last previous edition approved in 2009 as E1225 09. DOI: Standards volume information, refer to the standards Document Summary page on
10.1520/E1225-13. the ASTM website.

Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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E1225 13

T
Z
= absolute temperature (K),
= position as measured from the upper end of the
s 5 S
Z4 2 Z3 M T2 2 T1 T6 2 T5
1
T4 2 T3 2 Z2 2 Z1 Z6 2 Z5 D (1)

column, (m), This is a highly idealized situation, however, since it


l = specimen length, (m), assumes no heat exchange between the column and insulation
Ti = the temperature at Zi, (K),
at any position and uniform heat transfer at each meter
q' = heat flow per unit area, (W/m2),
, T, etc. = uncertainty in , T, etc., bar-specimen interface. The errors caused by these two as-
rA = specimen radius, (m), sumptions vary widely and are discussed in Section 10.
rB = guard cylinder inner radius, (m), and Because of these two effects, restrictions must be placed on this
Tg(z) = guard temperature as a function of position, z, test method, if the desired accuracy is to be achieved.
(K).
5. Significance and Use
4. Summary of Test Method 5.1 The comparative method of measurement of thermal
4.1 A test specimen is inserted under load between two conductivity is especially useful for engineering materials
similar specimens of a material of known thermal properties. A including ceramics, polymers, metals and alloys, refractories,
temperature gradient is established in the test stack and heat carbons, and graphites including combinations and other com-
losses are minimized by use of a longitudinal guard having posite forms of each.
approximately the same temperature gradient. At equilibrium 5.2 Proper design of a guarded-longitudinal system is diffi-
conditions, the thermal conductivity is derived from the mea- cult and it is not practical in a method of this type to try to
sured temperature gradients in the respective specimens and establish details of construction and procedures to cover all
the thermal conductivity of the reference materials. contingencies that might offer difficulties to a person without
4.2 General Features of Test Method: technical knowledge concerning theory of heat flow, tempera-
4.2.1 The general features of the guarded longitudinal heat ture measurements, and general testing practices. Standardiza-
flow technique are shown in Fig. 1. A specimen of unknown tion of this test method is not intended to restrict in any way the
thermal conductivity, S, but having an estimated thermal future development by research workers of new or methods or
conductance of S/ lS, is mounted between two meter bars of improved procedures. However, new or improved techniques
known thermal conductivity, M, of the same cross-section and must be thoroughly tested. Requirements for qualifying an
similar thermal conductance, M/lM. A more complex but apparatus are outlined in Section 10.
suitable arrangement is a column consisting of a disk heater
with a specimen and a meter bar on each side between heater 6. Requirements
and heat sink. Approximately one-half of the power would then 6.1 Meter Bar Reference Materials:
flow through each specimen. When the meter bars and speci- 6.1.1 Reference materials or transfer standards with known
men are right-circular cylinders of equal diameter the tech- thermal conductivities must be used for the meter bars. Since
nique is described as the cut-bar method. When the cross- the minimum measurement error of the method is the uncer-
sectional dimensions are larger than the thickness it is tainty in M, it is preferable to use standards available from a
described as the flat slab comparative method. Essentially, any National Metrology Institute. Other reference materials are
shape can be used, as long as the meter bars and specimen have available because numerous measurements of have been
the same conduction areas. made and general acceptance of the values has been obtained.
4.2.2 A force is applied to the column to ensure good Table 1 lists some of the recognized reference materials. Fig. 2
contact between specimens. The stack is surrounded by an shows the approximate variation of M with temperature.
insulation material of thermal conductivity, I. The insulation is 6.1.2 Table 1 is not exhaustive and other materials may be
enclosed in a guard shell with a radius, rB, held at the used as references. The reference material and the source of M
temperature, Tg(z). A temperature gradient is imposed on the values shall be stated in the report.
column by maintaining the top at a temperature, TT, and the 6.1.3 The requirements for any reference material include
bottom at temperature TB. Tg(z) is usually a linear temperature stability over the temperature range of operation, compatibility
gradient matching approximately the gradient established in with other system components, reasonable cost, ease of tem-
the test stack. However, an isothermal guard with Tg(z) equal to perature sensor attachment, and an accurately known thermal
the average temperature of the specimen may also be used. An conductivity. Since heat shunting errors for a specific I
unguarded system is not recommended due to the potential increase as M/s varies from unity, (1) the reference which has
very large heat losses, particularly at elevated temperatures a M nearest to S should be used for the meter bars.
(1).3 At steady state, the temperature gradients along the 6.1.4 If a samples thermal conductivity s is between the
sections are calculated from measured temperatures along the thermal conductivity values of two types of reference
two meter bars and the specimen. The value of S , as materials, the reference material with the higher M should be
uncorrected for heat shunting) can then be determined using used to reduce the total temperature drop along the column.
the following equation where the notation is shown in Fig. 1:
6.2 Insulation Materials:
6.2.1 A large variety of powder, particulate, and fiber
3
The boldface numbers in parentheses refer to a list of references at the end of materials exists for reducing both radial heat flow in the
this test method. column-guard annulus and surrounds, and for heat shunting

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E1225 13
along the column. Several factors must be considered during
selection of the most appropriate insulation. The insulation
must be stable over the anticipated temperature range, have a
low I, and be easy to handle. In addition, the insulation should
not contaminate system components such as the temperature
sensors, it must have low toxicity, and it should not conduct
electricity. In general, powders and particulates are used since
they pack readily. However, low density fiber blankets can also
be used.
6.2.2 Some candidate insulations are listed in Table 2.
6.3 Temperature Sensors:
6.3.1 There shall be a minimum of two temperature sensors
on each meter bar and two on the specimen. Whenever
possible, the meter bars and specimen should each contain
three sensors. The extra sensors are useful in confirming
linearity of temperature versus distance along the column, or
indicating an error due to a temperature sensor decalibration.
6.3.2 The type of temperature sensor depends on the system
size, temperature range, and the system environment as con-
trolled by the insulation, meter bars, specimen, and gas within
the system. Any sensor possessing adequate accuracy may be
used for temperature measurement (2) and be used in large
systems where heat flow perturbation by the temperature
sensors would be negligible. Thermocouples are normally
employed. Their small size and the ease of attachment are
distinct advantages.
6.3.3 When thermocouples are employed, they should be
fabricated from wires which are 0.1 mm diameter or less. A
FIG. 1(a) Schematic of a Comparative-Guarded-Longitudinal Heat Flow constant temperature reference shall always be provided for all
System Showing Possible Locations of Temperature Sensors cold junctions. This reference can be an ice-cold slurry (3), a
constant temperature zone box, or an electronic ice point
reference. All thermocouples shall be fabricated from either
calibrated thermocouple wire (4) or from wire that has been
certified by the supplier to be within the limits of error
specified in Table 1 of Standard E230.
6.3.4 Thermocouple attachment is important to this tech-
nique in order to ensure that reliable temperature measure-
ments are made at specific points. The various techniques are
illustrated in Fig. 3. Intrinsic junctions can be obtained with
metals and alloys by welding individual thermo-elements to the
surfaces (Fig. 3a). Butt or bead welded thermocouples junc-
tions can be rigidly attached by peening, cementing, or welding
in fine grooves or small holes (Fig. 3b, 3c, and 3d).
6.3.5 In Fig. 3b, the thermocouple resides in a radial slot,
and in Fig. 3c the thermocouple is pulled through a radial hole
in the material. When a sheathed thermocouple or a thermo-
couple with both thermoelements in a two-hole electrical
insulator is used, the thermocouple attachment shown in Fig.
3d can be used. In the latter three cases, the thermocouple
should be thermally connected to the solid surface using a
suitable glue or high temperature cement. All four of the
procedures shown in Fig. 3 should include wire tempering on
the surfaces, wire loops in isothermal zones, thermal wire
grounds on the guard, or a combination of all three (5).
6.3.6 Since uncertainty in temperature sensor location leads
FIG. 1(b) Schematic of Typical Test Stack and Guard System Illustrating to large errors, special care must be taken to determine the
Matching of Temperature Gradients correct distance between sensors and to calculate the possible
error resulting from any uncertainty.
FIG. 1

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TABLE 1 Reference Materials For Use as Meter Bars
Percentage
Temperature Thermal Conductivity
Material Uncertainty
Range (K) (W/mK)
( %)
Electrolytic IronA,B 2 to 1000 2 See Table 3.
TungstenC 4 to 300 2 See Table 4.
300 to 2000 2 to 5
>2000 5 to 8
Austenitic StainlessD 200 to 1200 <5 % See Table 5.
CopperE 85 to 1250 <2 M = 416.31 0.05904T + 7.0872
107/T3
PyroceramF,G,H,I,J,K 298 to 1025 K 6.5 = 2.332 + 515.2/T
4 for T > 300 K = 3.65367 6.64042 10-4
T 218.937T1 + 116163 T2
Fused SilicaL,M 1300 <8 M = (84.7 T) + 1.484 + 4.94 10 4
Up to 900 K T + 9.6 10 13T4
PyrexN,K,O,P,Q 90 to 600 <2 for T> 200 K = 1.1036 + 1.659 x 10-3 (T-273.15) 3.982
140 to 470 x 10-6 (T-273.15)2 + 6.746 x 10-9 (T-273.15)3
K
310 Stainless SteelK,R 300 to 1020 4 = 12.338 + 1.781 x 10-2 (T-273.15)
430 Stainless SteelK,R 300 to 770 4 = 20.159 + 1.589 x 10-2 (T-273.15) -1.283 x
-5
10 (T-273.15)2
Inconel 600S,K,R 300 to 1020 4 = 12.479 + 1.648 x 10-2 (T-273.15) + 3.741
x 10-6 (T-273.15)2
Nimonic 75T,K,R 300 to 1020 4 = 11.958 + 1.657 x 10-2 (T-273.15) + 3.252
x 10-6 (T-273.15)2
A
SRM 8420 is available from National Institute of Standards and Technology (NIST), Gaithersburg, MD.U
B
Hurst, J. G., and Lankford, A. B., Report of Investigation, Research Materials 8420 and 8421, Electrolytic Iron, Thermal Conductivity and Electrical Resistivity as a
Function of Temperature from 2 to 1000K, National Institutes of Standards and Technology (nee National Bureau of Standards), Gaithersburg, MD, 1984.
C
Hurst, J. G., and Giarratano, P. J., Certificate, Standard Reference Material 730, Thermal Conductivity Tungsten, National Institutes of Standards and Technology (nee
National Bureau of Standards), Gaithersburg, MD, 1976.
D
Hurst, J. G., Sparks, L. L., and Giaarratano, P. J., Certificate, Standard Reference Material 735, Thermal Conductivity Austenitic Stainless Steel, National Institutes
of Standards and technology (nee National Bureau of Standards), Gaithersburg, MD,USA, 1975.
E
Moore, J. P., Graves, R. S., and McElroy, D. L., Thermal Conductivity and Electrical Resistivity of High-Purity Copper from 78 to 400 K, Canadian Journal of Physics,
Vol 45, 1967, pp. 38493865.
F
Pyroceram is a trademark by Corning Incorporated, Corning, NY.
G
Salmon, D. R., Roebben, G., and Brandt,R., Certification of Thermal Conductivity and Thermal Diffusivity up to 1025 K of Glass-Ceramic Reference Material BCR-720,
EUR Report 21764, Institute for Reference Materials and Measurements (IRMM), Geel, Belgium, 2007.
H
Stroe, D. E., Thermitus, M. A., and Jacobs Fedore, R. A., Thermophysical Properties of Pyroceram 9606, Thermal Conductivity 27 / Thermal Expansion 15, H.
Wang, W. Porter, eds., DEStech Publications, Lancaster, PA, 2005, pp. 382390.
I
BCR-2013 is available from the Institute for Reference Materials and Measurements (IRMM), Geel, Belgium.U
J
BCR-724 is available from the Laboratory of the Government Chemists (LGC), Teddington, Middlesex, UK.U
K
Tye, R. P., and Salmon, D. R., Development of New Thermal Conductivity Reference Materials: A Summary of Recent Contributions by National Physical Laboratory,
Thermal Conductivity 27/ Thermal Expansion 15, H. Wang (ed.), DEStech Publications, Lancaster PA, 2005, pp. 372381.
L
Above 700 K a large fraction of heat conduction in fused silica will be by radiation and the actual effective values may depend on the emittances of bounding surfaces
and meter bar size.
M
Recommended values from Table 3017 A-R-2 of the Thermophysical Properties Research Center Data Book, Vol. 3, Nonmetallic Elements, Compounds, and Mixtures,
Purdue University, Lafayette, Indiana.
N
Pyrex is a trademark by Corning Incorporated, Corning, NY.
O
Tye, R. P., and Salmon, D. R., Thermal Conductivity Certified Reference Materials: Pyrex 7740 and Polymethylmethacrylate, Thermal Conductivity 26 / Thermal
Expansion 14, R. Dinwiddie, ed., DEStech Publications, Lancaster, PA, 2005, pp. 437451.
P
BCR-39 is available from the Institute for Reference Materials and Measurements (IRMM), Geel, Belgium.U
Q
Salmon, D., Thermal Conductivity of Insulations Using Guarded Hot Plates, including Recent Developments and Sources of Reference Materials, Measurement
Science and Technology, Vol 12, 2001, pp. R89R98.
R
Clark, J., and Tye, R., Thermophysical Properties Reference Data for Some Key Engineering Alloy, High Temperatures High Pressures, Vols 35/36, 2003/2004, pp.
114.
S
Inconel is a trademark by Special Metals Corporation, Huntington WV.
T
Nimonic is a trademark by Special Metals Corporation, Huntington WV.
U
This is the sole source of supply of this material known to the committee at this time. If you are aware of alternative suppliers, please provide this information to ASTM
International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend.

6.4 Reduction of Contact Resistance: 6.4.2 For the relatively thin specimens normally used for
6.4.1 This test method requires uniform heat transfer at the materials having a low thermal conductivity, the temperature
meter bar to specimen interfaces whenever the temperature sensors must be mounted close to the surface and in conse-
sensors are within a distance equal to rA from an interface (6). quence the uniformity of contact resistance is critical. In such
This requirement necessitates a uniform contact resistance cases, a very thin layer of a compatible highly conductive fluid,
across the adjoining areas of meter bars and specimens. This is paste, soft metal foil, or screen shall be introduced at the
normally attained by use of an applied axial load in conjunction interfaces.
with a conducting medium at the interfaces. Measurements in 6.4.3 Means shall be provided for imposing a reproducible
a vacuum environment are not recommended, unless the and constant load along the column with the primary purpose
vacuum is required for protection purposes. of minimizing interfacial resistances at meter bar-specimen

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TABLE 2 Suitable Thermal Insulation Materials TABLE 4 Thermal Conductivity of TungstenA
Typical Thermal Conductivity (W/(mK)) Temperature, Thermal Conductivity,
MaterialA K (W/mK)
300K 800K 1300K
4 154
Poured Powders 6 231
Diatomaceous Earth 0.053 0.10 0.154 8 306
Bubbled Alumina 0.21 0.37 0.41 10 377
Bubbled Zirconia 0.19 0.33 0.37 12 444
Vermiculite 0.07 0.16 ... 14 503
Perlite 0.050 0.17 ... 16 553
Blankets and Felts 18 591
Aluminosilicate 60120 kg/m3 0.044 0.13 0.33 20 618
Zirconia 6090 kg/m3 0.039 0.09 0.25 30 585
A
All materials listed can be used up to the 1300 K limit of the comparative 40 438
longitudinal except where noted. 50 330
60 275
70 245
80 229
TABLE 3 Thermal Conductivity of Electrolytic IronA 90 218
Temperature, Thermal Conductivity, 100 211
K (W/mK) 120 202
2 12.32 140 197
3 18.48 160 194
4 24.62 180 190
5 30.76 200 187
6 36.88 250 180
7 42.97 300 172
8 49.0 350 164
9 55.0 400 157
10 61.0 450 151
12 72.8 500 146
14 84.2 600 138
16 95.2 700 132
18 105.7 800 127
20 115.7 900 123
25 137.4 1000 120
30 153.9 1200 114
35 164.5 1400 110
40 169.1 1600 107
45 168.3 1800 105
50 163.6 2000 102
60 149.1 2200 101
70 134.9 2400 99
80 123.8 2600 98
90 115.4 2800 97
100 108.9 3000 97
150 92.7 A
Hurst, J. G., and Giarratano, P. J., Certificate, Standard Reference Material 730,
200 86.7 Thermal Conductivity Tungsten, National Institute of Standards and Technology
250 81.5 (nee National Bureau of Standards), 1976.
300 76.4
400 67.5
500 60.2
600 53.6 errors caused by poor contact, by judicious positioning of
700 47.49
800 41.96 temperature sensors away from any heat flow perturbation at
900 37.12 the interfaces.
1000 32.98
A
6.5 Guard Cylinder:
Hurst, J. G., and Lankford, A. B., Report of Investigation, Research Materials
8420 and 8421, Electrolytic Iron, Thermal Conductivity and Electrical Resistivity as 6.5.1 The specimen-meter bar column shall be enclosed
a Function of Temperature from 2 to 1000K, National Institute of Standards and within a guard tube or pipe normally of right circular symme-
Technology (nee Bureau of Standards), 1984.
try. This guard cylinder can be either a metal or a ceramic but
its inside radius should be such that the ratio rB/rA will be
between 2.0 and 3.5 (1). This guard cylinder shall contain at
interfaces. Since the force applied to the column usually affects least one heater for controlling the temperature profile along
the contact resistance, it is desirable that this force be variable the guard.
to ensure that S does not change with force variation. This 6.5.2 The guard shall be constructed and operated so that the
force can be applied either pneumatically, hydraulically, by temperature of the guard surface is either isothermal and equal
spring action, or by putting a dead weight on the column. The to the approximate mean temperature of the specimen or
above load mechanisms have the advantage of remaining preferably has an approximately linear profile with the top and
constant with change in column temperature. In some cases, bottom ends of the guard matched to corresponding positions
the compressive strength of the specimen might be so low that along the column. In each case, at least three temperature
the applied force must be limited to the dead weight of the sensors shall be attached to the guard at known positions to
upper meter bar. In this case, special care must be taken to limit measure the temperature profile.

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TABLE 5 Thermal Conductivity of Austenitic Stainless SteelA
Temperature, Thermal Conductivity,
K (W/mK)
5 0.466
6 0.565
7 0.676
8 0.796
9 0.921
10 1.05
12 1.32
14 1.58
16 1.86
18 2.13
20 2.40
25 3.07
30 3.72
35 4.34
40 4.92
45 5.47
50 5.98
55 6.45
60 6.88
65 7.28
70 7.64
75 7.97
80 8.27
85 8.55
90 8.80
95 9.04
100 9.25
110 9.65
120 9.99
130 10.3
140 10.6
150 10.9
160 11.1
170 11.4
180 11.6
190 11.9 NOTE 1The material selected for the meter bars should have a thermal
200 12.1 conductivity as near as possible to the thermal conductivity of the
250 13.2 unknown.
300 14.3 FIG. 2 Approximate Values for the Thermal Conductivity of Sev-
350 15.3 eral Possible Reference Materials for Meter Bars
400 16.2
450 17.1
500 17.9
600 19.3 7. Sampling and Conditioning Test Specimens
700 20.6
800 21.9
7.1 Test SpecimensThis test method is not restricted to a
900 23.0 particular geometry. General practice is to use cylindrical or
1000 24.1 square cross-sections. The conduction area of the specimen and
1100 25.1
1200 26.1
reference samples must be the same to within 1 % (see Note 3)
A
and any difference in area shall be taken into account in the
Hurst, J. G., Sparks, L. L., and Giarratano, P. J., Certificate, Standard Reference
Material 735, Thermal Conductivity Austenitic Stainless Steel, Thermal Con- calculations of the result. For the cylindrical configuration, the
ductivity as a Function of Temperature (5 to 1200 K), National Institute of radii of the specimen and meter bars must agree to within
Standards and Technology (nee National Bureau of Standards), 1975. 61 % and the specimen radius, rA, must be such that rB/rA is
between 2.0 and 3.5. Each flat surface of the specimen and
reference must be flat with a surface finish equal to or better
than 32 and the normal to each end shall be parallel with the
6.6 System Instrumentation: specimen axis to within 610 min.
6.6.1 The combination of temperature sensor and the instru- NOTE 3In some cases this requirement is not necessary. For example,
ment used for measuring the sensor output shall be adequate to some apparatus might consist of meter bars and specimen with high values
ensure a temperature measurement precision of 60.04 K and of M and S so that thermal shunting errors would be small for long
sections. These sections might be long enough to permit temperature
an absolute error less than 60.5 %. sensor attachment to be far enough away from the interfaces to ensure that
6.6.2 Instrumentation for this technique shall be adequate to heat flow was uniform. The specimen length should be selected based on
maintain the required temperature control and measure all considerations of radius and thermal conductivity. When M is higher than
pertinent output voltages with accuracy commensurate with the the thermal conductivity of stainless steel, long specimens with length / rA
system capability. Although control can be manual, a technique >>1 can be used. These long specimens permit the use of large distances
between temperature sensors and this reduces the percentage error derived
of this general description can be automated so that a computer from the uncertainty in sensor position. When M is lower than the thermal
carries out all the control functions, acquires all pertinent conductivity of stainless steal, the samples length must be reduced
voltages, and calculates the thermal conductivity (7). because uncertainty due to the heat shunting becomes too large.

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3a 3b
Intrinsic weld with separate temperature elements welded to specimen or meter Radial slots on the flat surfaces to hold a bare wire or ceramic insulated
bars so that signal is through the material. thermocouple sensor the may be bonded into slot.

3c 3d
Small radial hole drilled through the specimen or meter bar and non-insulated Small Radial hole drilled part way through the specimen or meter bar and a
(permitted if the material is an electrical insulator) or insulated thermocouple pulled thermocouple pushed into the hole.
through the hole.

NOTE 1In all cases the thermoelements should be thermally tempered or thermally grounded on the guard, or both, to minimize temperature
measurement errors due to heat flow into or out of the hot junction.
FIG. 3 Thermocouple Attachments

7.2 Sampling and ConditioningUnless specifically re- ence material which has the closest to that of the specimen.
quired or prescribed, one representative specimen shall be For example, verification tests might be performed on a
prepared from the sample. Pyroceram4 specimen using meter bars fabricated from stain-
less steel. If the measured thermal conductivity of the specimen
8. Calibration and Verification disagrees with the value from Table 1 after applying the
8.1 There are many situations that call for equipment corrections for heat exchange, additional effort is required to
verifications before operations on unknown materials can be find the error source(s).
successfully accomplished. These include the following:
8.1.1 After initial equipment construction, 9. Procedure
8.1.2 When the ratio of M to S is less than 0.3 or greater 9.1 Where possible and practical, select the reference speci-
than 3 and it is not possible to match thermal conductance mens (meter bars) such that the thermal conductance is of the
values, same order of magnitude as that expected for the test specimen.
8.1.3 When the specimen shape is complex or the specimen After instrumenting and installing the proper meter bars, the
is unusually small, specimen should be instrumented similarly. It should then be
8.1.4 When changes have been made in the system inserted into the test stack such that it is at aligned between the
geometry, meter bars with at least 99 % of each specimen surface in
8.1.5 When meter bar or insulation material other than those contact with the adjacent meter bar. Soft foil or other contact-
listed in 5.1 and 5.2 are considered for use, and ing medium may be used to reduce interfacial resistance. If the
8.1.6 When the apparatus has been previously operated to a system must be protected from oxidation during the test or if
high enough temperature to change the properties of a compo- operation requires a particular gas or gas pressure to control I,
nent such as thermocouples sensitivity. the system should be pumped and purged, and the operating
8.2 These verification tests shall be run by comparing at gas and pressure established. The predetermined force required
least two reference materials in the following manner: for reducing the effects of non-uniform interfacial resistance
8.2.1 A reference material which has the closest thermal should be applied to the load column.
conductivity to the estimated thermal conductivity of the 9.2 Heaters at either end of the column should be energized
unknown sample should be machined according to 6.1, and (see Note 4) and adjusted until the temperature differences
8.2.2 The thermal conductivity of the specimen fabricated
from a reference material shall then be measured as described
in Section 9, using meter bars fabricated from another refer- 4
Pyroceram is a trademark by Corning Incorporated, Corning, NY.

7
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between positions Z1 and Z2, Z3 and Z4, and Z5 and Z6 are 10.2.1 Calculation of the specimen thermal conductivity by
between 200 times the imprecision of the T measurements a simple comparison of temperature gradients in the meter bars
and 30 K, and the specimen is at the average temperature to that in the specimen is less valid when the specimen or meter
desired for the measurement. Although the exact temperature bars, or both, have low thermal conductivities relative to that of
profile along the guard is not important for rB/rA 3, the power the insulation. The apparatus should be designed to minimize
to the guard heaters should be adjusted until the temperature these errors. The deviation from uniform heat flow has been
profile along the guard, Tg(z), is constant with respect to time expressed as follows (1):
to within 60.1 K and either: 5 F gF (5)
9.2.1 Approximately linear so that Tg(z) coincides with the
temperature along the sample column at a minimum of three where Fg is a function of system dimensions, and F is a
places including the temperature at the top sensor on the top function of M, I, and S (1). The Fg term has a value between
meter bar, the bottom sensor on the bottom bar, and the 2 and 3 for the ratio of guard radius to column radius specified
specimen midplane; or for this system. The F term is shown in Fig. 4 as a function of
/I for various values of M/I for a linear guard. At high ratios
9.2.2 Constant with respect to z to within 65 K and
of M/I and S/I, corrections would not be necessary since the
matched to the average temperature of the test specimen.
departure from ideal heat flow would be small. For example,
NOTE 4These heaters can either be attached to the ends of the meter the product of F and Fg would be less than 0.10 (10 %) for all
bars or to a structure adjacent to the meter bar. The heaters can be powered measurements where M/I and S/I are greater than 30. If the
with alternating or direct current. The power to these heaters shall be value of FgF is to be kept below 10 %, the ratios M/I and
steady enough to maintain short term temperature fluctuations less than
60.03 K on the meter bar temperature sensor nearest the heater. These two
s/I must be within the boundaries on Fig. 4.
heaters, in conjunction with the guard shell heater and the system coolant 10.2.2 Measurements on materials where the ratios of M/I
shall maintain long term temperature drift less than 60.05 K/h. and S/I do not fall within these boundaries shall be accom-
panied with corrections for extraneous heat flow. These cor-
9.3 After the system has reached steady state (T drift <0.05
rections can be determined in the following three different
K/h), measure the output of all temperature sensors.
ways:
10.2.2.1 Use of analytical techniques as described by
10. Calculation
Didion (1) and Flynn (8),
10.1 Approximate Specimen Thermal Conductivity: 10.2.2.2 Using calculations from finite-difference or finite-
10.1.1 The outputs from the temperature sensors shall be element heat conduction codes, and
converted to temperature, and the apparent heat flow per unit 10.2.2.3 Determined experimentally by using several refer-
area, q', in the meter bars shall be calculated using the ence materials or transfer standards of different thermal con-
following: ductance as specimens. The procedure must be used cautiously
since all such specimens should have the same size as the
T2 2 T1
q' T 5 M (2) specimen with an unknown thermal conductivity and have the
Z2 2 Z1
same surface finish.
top bar
T6 2 T5
q' B 5 M (3)
Z6 2 Z5

bottom bar

In each of these equations, the M value (see Note 5) to be


inserted shall be obtained from the information of 6.1 for the
average meter bar temperature. Although these two values, q'T
and q'B, should agree with each other to within about 610 %
when heat exchange with the insulation is small, good agree-
ment is not a sufficient condition (nor always a necessary
condition) for low heat shunting error.
10.1.2 A value for the specimen thermal conductivity at
temperature (T3 + T4)/2, as uncorrected for heat exchange with
the insulation, can then be calculated using the following:
~ q' T 1q' B ! ~ Z 4 2 Z 3 !
' S 5 (4)
2 ~ T 4 2 T 3!
NOTE 5This type of calculation procedure actually requires only two
temperature sensors on each column section. In this case, the third sensor
on each section serves as a test for consistency of the other two. Some s/i
calculation procedures require more than the two sensors to obtain more
knowledge about the temperature gradient dT/dZ. FIG. 4 Fractional Heat Exchange Between the Meter Bar-
Specimen Column and Surrounding Insulation as a Function of
10.2 Corrections for Extraneous Heat Flow: m/i for Several Values of s/i

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E1225 13
11. Report T 2 2 T 1 ;T 4 2 T 3 ;T 6 2 T 5 5 10 K;
11.1 The report of the test results shall include the follow-
~Z2 2 Z 1 ! ; ~ Z 4 2 Z 3 ! ; ~ Z 6 2 Z 5 ! 5 0.2 mm; and
ing:
11.1.1 Complete specimen identification including shape ~T2 2 T 1 ! ; ~ T 4 2 T 3 ! ; ~ T 6 2 T 5 ! 5 0.04 K.
and size;
11.1.2 Complete identification of insulation and source of I 12.1.2 The maximum value of (Z2 Z1) etc. was approxi-
values, gas, and gas pressure; mated by assuming an uncertainty of 60.5 (sensor diameter) at
11.1.3 Statements of temperature sensor type, size, and each temperature measurement position. Therefore, if the
attachment procedure; diameter of each sensor is 0.2 mm, the uncertainty in the
11.1.4 Complete listing of the geometrical dimensions of difference would be 60.2 mm. The number for (T2 T1) etc.
the system including r A, rB, specimen height, meter bar height, was calculated based on the sensor absolute accuracy.
and distances between temperature sensors;
11.1.5 Column force; 12.1.3 With these values the fractional uncertainty in 'S
11.1.6 Meter bar material and source of M values if other will be |0.069| or 66.9 %.
than those listed in Table 1; 12.2 Indeterminate Errors:
11.1.7 Reference to the use of this test method shall include 12.2.1 There are at least three other errors that can contrib-
a statement of the percentage variation of the qualification
ute to total system error and these are (1) non-uniform
results about the true value. For example, thermal conductiv-
interfacial resistance, (2) heat exchange between the column
ity results on Pyroceram using stainless steel meter bars were
and the guard, and (3) heat shunting through the insulation
within 64 % of the accepted values for Pyroceram over the
temperature range from 250 to 900 K; around the column. These three errors must be minimized or
11.1.8 Variations, if any, from this test method. If results are appropriate corrections applied to the data if the desired
to be reported as having been obtained by this method, then all accuracy is to be obtained.
requirements prescribed by this method shall be met. Where 12.2.2 The contributions from the last two errors can be
such conditions are not met, the phrase, All requirements of determined approximately using results from appropriate ex-
this method have been met with the exception of ... shall be periments carried out at different levels of guard temperature to
added and a complete list of the exceptions included; specimen stack temperature out of balance.
11.1.9 Measured values of temperature and specimen ther-
12.3 OverallAn international, inter-laboratory round
mal conductivity; and
11.1.10 The specific dated version of this standard used. robin study also involving absolute methods (9, 10) has shown
that a precision of 66.8 % can be attained over the temperature
12. Precision and Bias range 300 to 600 K. Although no definite bias could be
12.1 Example of Error Estimation: established these are indications that the values were on the
12.1.1 Assumptions for a system where both meter bars and order of 2 % lower than those obtained by absolute methods.
the specimen are of equal length is that the sensor spacings are This cited paper is on file at ASTM as a research report.5
all 13 mm and M S:

U U
M
M ?
5 0.003 ? (6)
5
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:E37-1010. Contact ASTM Customer
Z 2 2 Z 1 ;Z 4 2 Z 3 ;Z 6 2 Z 5 5 13 mm; Service at service@astm.org.

REFERENCES

(1) Didion, D. A., An Analysis and Design of a Linear Guarded Cut-Bar (4) American Society of Mechanical Engineers (ASME): PTC 19.3,
Apparatus for Thermal Conductivity Measurements, AD-665789, Temperature Measurement, Part 3, 1974, p. 1232.
January, 1968, available from the National Technical Information (5) Anderson, R. L., and Kollie, T. G., Problems in High Temperature
Service, Springfield, VA. Thermometry, CRC Critical Reviews in Analytical Chemistry, Vol 6,
(2) Finch, D. I., General Principles of Thermoelastic Thermometry, 1976, pp. 171221.
Temperature, Its Measurement and Control in Science and Industry, (6) Fried, E., Thermal Conduction Contribution to Heat Transfer at
Vol. 3, Part 2, Section 1, Reinhold Publishing Corporation, 1962, pp. Contacts, Thermal Conductivity, Vol 2, Tye, R. P., ed., Academic
331. Press, New York, 1969, pp. 253274.
(3) Caldwell, F. R., Temperatures of Thermocouple Reference Junctions (7) Morgan, M. T., and West, G. A., Thermal Conductivity of the Rocks
in an Ice Bar, Journal of Research of the National Bureau of in the Bureau of Mines Standard Rock Site, Thermal Conductivity
Standards, Vol 69C, No. 2, 1965, pp. 95101. 16, Larsen, D. C., ed., Plenum Press, New York, 1983, pp. 7990.

9
E1225 13
(8) Flynn, D. R., Thermal Conductivity of Ceramics, Mechanical and (10) Hulstrom, l. C., Interlaboratory Comparison Testing of Thermal
Thermal Properties of Ceramics, Special Publication 303, National Conductivity Reference Materials to 573 K; A Progress Report,
Bureau of Standards, 1969, pp. 63123. High Temperatures-High Pressures, Vol 17, 1985, pp. 707708.
(9) Hulstrom, L. C., Tye, R. P., and Smith, S. E., Round-Robin Testing
of Thermal Conductivity Reference Materials, Thermal Conductivity
19, Yarbrough, D. W., ed., Plenum Press, New York, 1985, pp.
199211.

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